The Use of Microwave Assisted Extraction and On-line Chromatography-Mass Spectrometry for Determining Endocrine-Disrupting Compounds in Sewage Sludges

  • T. Vega-Morales
  • Z. Sosa-Ferrera
  • J. J. Santana-Rodríguez
Article

Abstract

A new analytical methodology based on ultra high performance liquid chromatography (UHPLC) after microwave assisted extraction, followed by a clean-up and preconcentration step with solid phase extraction (MAE–SPE) has been developed for the simultaneous determination of 11 endocrine-disrupting compounds (EDCs), including alkylphenolic compounds, bisphenol A, and various synthetic and natural steroidal hormones, in sewage sludge samples. The effects of different variables on MAE-SPE were studied and optimised. The recoveries obtained were higher than 77 %, whereas the relative standard deviations were less than 9 %. The detection limits ranged between 0.1 and 0.7 ng g−1. The developed methodology was successfully applied to the assessment of the presence of EDCs to sewage sludge samples that were collected bimonthly during 1 year and a half from two wastewater treatment plants (WWTPs) located in Las Palmas de Gran Canaria (Canary Islands, Spain). All compounds were consistently found in all the samples under study.

Keywords

Endocrine-disrupting UHPLC Mass spectrometry Microwave assisted extraction Sludge samples Factorial design 

References

  1. Baillie, H. S., Pacey, A. A., & Moore, H. D. M. (2002). Environmental chemical and the threat to male fertility in mammals: evidence and perspective. Reproductive Science and Integrated Conservation, Conservation Biology, 8, 57–65.CrossRefGoogle Scholar
  2. Benijts, T., Dams, R., Lambert, W., & De Leenheer, A. (2004). Countering matrix effects in environmental liquid chromatography–electrospray ionization tándem mass spectrometry water analysis for endocrine disrupting chemicals. Journal of Chromatography. A, 1029, 153–159.CrossRefGoogle Scholar
  3. Cooper, R. L., & Kavlock, R. J. (1997). Endocrine disruptors and reproductive development: a weight-of-evidence overview. Journal of Endocrinology, 15, 159–166.CrossRefGoogle Scholar
  4. Eskilsson, C., & Björklund, E. (2000). Analytical-scale microwave-assisted extraction. Journal of Chromatography A, 902, 227–250.CrossRefGoogle Scholar
  5. Fisher, J. S. (2004). Are all EDC effects mediated via steroid hormone receptors? Toxicology, 205, 33–41.CrossRefGoogle Scholar
  6. Fountoulakis, M., Drillia, P., Pakou, C., Kampioti, A., Stamatelatou, K., & Lyberatos, G. (2005). Analysis of nonylphenol and nonylphenol ethoxylates in sewage sludge by high performance liquid chromatography following microwave-assisted extraction. Journal of Chromatography A, 1089, 45–51.CrossRefGoogle Scholar
  7. Gabet-Giraud, V., Miege, C., Herbreteau, B., Hernandez-Raquet, G., & Coquery, M. (2010). Development and validation of an analytical method by LC-MS/MS for the quantification of estrogens in sewage sludge. Analytical and Bioanalytical Chemistry, 396, 1841–1851.CrossRefGoogle Scholar
  8. Geyer, H.J., Rimkus, G.G., Scheunert, I., Kaune, A., Schramm, K.W., Kettrup, A., et al. (2000). Bioaccumulation and occurrence of endocrine-disrupting chemicals (EDCs), persistent organic pollutants (POPs), and other organic compounds in fish and other organisms including humans. The Handbook of Environmental Chemistry. Heidelberg: Springer.Google Scholar
  9. Hammes, B., & Laitman, C. J. (2003). Diethylstilbestrol (DES) update: recommendations for the identification and management of DES-exposed individuals. Journal of Midwifery & Women’s Health, 48, 19–29.CrossRefGoogle Scholar
  10. Kamata, R., & Masatoshi, M. (2002). Disrupting Chemicals and Reproductive Disorder in Birds. Journal of Environmental Chemistry, 12, 23–31.CrossRefGoogle Scholar
  11. Kavlock, R. J. (1999). Overview of endocrine disruptor research activity in the United States. Chemosphere, 39, 1227–1236.CrossRefGoogle Scholar
  12. Kavlock, R. J., & Ankley, G. T. (1996). A perspective on the risk assessment process for endocrine-disruptive effects on wildlife and human health. Risk Analysis, 16, 731–739.CrossRefGoogle Scholar
  13. Kavlock, R. J., Daston, G. P., DeRosa, C., Fenner-Crisp, P., Gray, L. E., Kaattari, S., et al. (1996). Research needs for the risk assessment of health and environmental effects of endocrine disruptors: a report of the U.S. EPA-sponsored workshop. Environmental Health Perspectives, 104, 715–740.Google Scholar
  14. Lai, K. M., Johnson, K. L., Scrimshaw, M. D., & Lester, J. N. (2000). Binding of waterborne steroid estrogens to solid phases in river and estuarine systems. Environmental Science & Technology, 34, 3890–3894.CrossRefGoogle Scholar
  15. Matuszewski, B. K., Constanzer, M. L., & Chavez-Eng, C. M. (2003). Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS. Analytical Chemistry, 75, 3019–3030.CrossRefGoogle Scholar
  16. Mei, H., Hsieh, Y. S., Nardo, C., Xu, X. Y., Wang, S. Y., Ng, K., et al. (2003). Investigation of matrix effects in bioanalytical high-performance liquid chromatography/tandem mass spectrometric assays: application to drug discovery. Rapid Communications in Mass Spectrometry, 17, 97–103.CrossRefGoogle Scholar
  17. Miller, J., & Miller, J. (2005). Statistics and Chemometrics for Analytical Chemistry, fifth ed. Pearson Education Limited, Prentice Hall Ptr., Harlow.Google Scholar
  18. Pinto, B., Garritano, S., & Reali, D. (2001). Occurrence of estrogen-like substances in the marine environment of the Northern Mediterranean Sea. Marine Pollution Bulletin, 50, 1681–1685.CrossRefGoogle Scholar
  19. Pojana, G., Gomiero, A., Jonkers, N., & Marcomini, A. (2007). Natural and synthetic endocrine disrupting compounds (EDCs) in water, sediment and biota of a coastal lagoon. Environmental International, 33, 929–936.CrossRefGoogle Scholar
  20. Porte, C., Janer, G., Lorusso, L. C., Ortiz-Zarragoitia, M., Cajaraville, M. P., Fossi, M. C., et al. (2006). Endocrine disruptors in marine organisms: approaches and perspectives. Comparative Biochemistry and Physiology Part C: Toxicology & Pharmacology, 143, 303–315.CrossRefGoogle Scholar
  21. Sonnenschein, C., & Soto, A. M. (1998). An updated review of environmental estrogen and androgen mimics and antagonists. The Journal of Steroid Biochemistry and Molecular Biology, 65, 143–150.CrossRefGoogle Scholar
  22. Souverain, S., Rudaz, S., & Veuthey, J. L. (2004). Matrix effect in LC-ESI-MS and LC-APCI-MS with off-line and on-line extraction procedures. Journal of Chromatography A, 1058, 61–66.Google Scholar
  23. Tabb, M. M., & Blumberg, B. (2006). New modes of action for endocrine-disrupting chemicals. Molecular Endocrinology, 20, 475–482.CrossRefGoogle Scholar
  24. Vega-Morales, T., Sosa-Ferrera, Z., & Santana-Rodríguez, J. J. (2010). Determination of alkylphenol polyethoxylates, bisphenol-A, 17α-ethynylestradiol and 17β-estradiol and its metabolites in sewage samples by SPE and LC/MS/MS. Journal of Hazardous Materials, 183, 701–711.CrossRefGoogle Scholar
  25. Vega-Morales, T., Sosa-Ferrera, Z., & Santana-Rodríguez, J. J. (2011). Determination of various estradiol mimicking-compounds in sewage sludge by the combination of microwave-assisted extraction and LC-MS/MS. Talanta, 85, 1825–1834.CrossRefGoogle Scholar
  26. Vega-Morales, T., Sosa-Ferrera, Z., & Santana-Rodríguez, J. J. (2012). Development and optimisation of an on-line solid phase extraction coupled to ultra-high-performance liquid chromatography–tandem mass spectrometry methodology for the simultaneous determination of endocrine disrupting compounds in wastewater samples. Journal of Chromatography A, 1230, 66–76.CrossRefGoogle Scholar
  27. Ying, G. G., & Kookana, R. (2003). Degradation of five selected endocrine-disrupting chemicals in seawater and marine sediment. Environmental Science and Technology, 37, 1256–1260.CrossRefGoogle Scholar
  28. Ying, G. G., & Kookana, R. (2005). Sorption and degradation of estrogen-like-endocrine disrupting chemicals in soil. Environmental Toxicology and Chemistry, 24, 2640–2645.CrossRefGoogle Scholar
  29. Ying, G. G., Williams, B., & Kookana, R. (2002). Environmental fate of alkylphenols and alkylphenol ethoxylates — a review. Environmental International, 28, 215–226.CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media Dordrecht 2013

Authors and Affiliations

  • T. Vega-Morales
    • 1
  • Z. Sosa-Ferrera
    • 1
  • J. J. Santana-Rodríguez
    • 1
  1. 1.Departamento de QuímicaUniversidad de Las Palmas de Gran CanariaLas Palmas de Gran CanariaSpain

Personalised recommendations